Mesoporous nanocrystalline Cd-doped titania was firstly prepared at low temperature by a modified sol-gel method, using dodecylamine as a template. The template could be easily removed by refluxing samples in nitric acid ethanol solution. The Fourier transform infrared spectrometer (FT-IR), low-angle and wideangle X-ray diffraction (XRD), N 2 adsorption-desorption, transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS), and UV-visible diffuse reflectance spectroscopy were used for the characterization of catalysts. The characteristic results clearly showed that Cd 2? ions were doped into the titania lattice, and the mesoporous architecture of Cd-doped TiO 2 was composed of mixed-phase crystal textures of anatase and brookite. The samples displayed high visible-light photocatalytic activity for photodegradating 2,4-dichlorophenol (2,4-DCP) solution. The high activities of samples were attributed to the bicrystalline framework, large BET surface area, small crystallite size, and Cd-doping.